Fabriken



PHILIP? oTT, or ELBERFELD, GERMANY, AssIeNoR'ro THE FARBEN- FABRIKEN,VORMALS FR. BAYER & 00., OF SAME PLACE.

SPECIFICATION formingpart of Letters Patent a0. 48,405, dated May so,1893.

Application filed January 26, 1893, Serial No. 459.911. (Specimena)Patented in France April 28; 1892, No. 221,233, m1- in Italy June 24;1892, XXVI, No, 32,191. 7

To all whom it may-camera.-

Be it known that I, PHIIJIPP ()T'l, doctor of philosophy, chemist,(assign-or to FARBENFAB- RIKEN, VO'RMALS Fa.- BAYER & 00.,01" Elber=feld, Germany) a subject of the Emperor of Germany, residing atElberfeld, Germany,

have invented a new and useful'linprovement in: theManufac'tiire ofDye-Stuffs, (for which the aforesaid FARBENFABRIKEN has already obtainedLetters Patent in the following countries: France, No. 221,233, datedApril 28,1892, and Italy; Vol; XXVI, No. 32,191, dated June 24, 1892,)of which the following is a specifi cation; i I

My invention relates to the product-ion of a new disa'zo coloring-matterby combining one molecular proportion of diazo benzene chlo ride oranother diaz'o benzene salt, with one molecular proportion of the socalled. Cleves alphanaphthylainine betanionosulpho acid beta or deltaor. a soluble salt thereof (de scribed in the Bulletin de la SocitOhimt'que, Vol. 26,page 447, and Bemlchte der Deutschen OhemischenGesellschafl, Vol. 21, page 3264,) by rediazotizing the so formedamidoazo compound and coupling the resulting diazo derivative with onemolecular proportion of phenylnapthylamine sulpho acid derived fromalphanapthylamiue alpha 'monosulpho acid (1:8).

The phenylnaphthylamine monosulpho acid, which I employ, can be obtainedby heating alphanaphthylamine alpha monosulpho acid (1:8) with anilineand a salt thereof, for instance, by heating one part, by weight, of thesaid alpha naphthylamine alpha monosulpho acid (1:8) with three to fiveparts, by weight, of aniline and one part, by weight, of anilinehydrochlorate at from about 160 to 170 centigrade for about ten hours,treating the resulting mixture, when cooled, with diluted hydrochloricacid,boiling the separated acid, after filtering off, with a dilutedsolution of sodium carbonate in excess in order to remove the excess ofaniline, filtering the alkaline solution, acidulating the filtrateobtained by means of amineral acid and isolating the free acid separatedby filtering off, pressing and drying.

In carrying out my process practically I aniline or thecorrespondingquantity of a soluble salt thereof are diazotizcd in theusual manner by means of 0 7 kilos; by weight, of sodium nitrite inhydrochloricsolution. The resulting diazo solutionis allowed to flowinto a watery solution of 2415 kilos-by "Weight, of the sodium salt ofQl'eves alphanaphthfylamine beta monosulplioacid (betafo'r delta acid)and about five kilos, by weight, of sopioceea as jiollowsi 0,93 kilos,by weight, or

'di'uni acetate, In oide'rto complete the reaetion, the mixture isheated after somedays for a short time at from about to ceti= tigra'd'e.After rendering alkaline by the addition of sodium carbonateer-soda-lyeth resuiting amidoazo product is filtered 01f; The latter ismixed with a small quantityof water and, {after adding a concentratedsolution in water of 0.7 kilos, by weight, er sjo'diuin' iii trite;hydrochloric acid is slowlyadd'ed, until the liquid mixture shows alasting acid reac'-" tion. In this manner the diazo derivative of theabove amidoazo product is formed. The resulting mixture is introducedinto a'watery solution of 6.4kilos,by weight, of sodiumacetate and 3.21kilos,- by weight, of the sodium salt of phenylalphanaphthylamine alphamonosulpho acid which is derived from alphanaphthylamine My newdye-stuff having the following com-v position:

forms after drying and pulverizing an oliveblack powder showing metallicluster. It is soluble in water with dark Violet color and dissolvesinalcohol with blue color. By ammonia itis dissolved with blue color. Itis almost insoluble in sodium carbonate and soda-lye, even on heating.In diluted hydro- IOO chloric and sulfuric acid it is insoluble. Onadding to its watery solutions ammonia or sodium carbonate the color isnot changed, while an excess of these two reagents causes the separationof blue or reddish-blue flakes. When soda-lye is added to its solutionsin water, the liquid gradually becomes dull, and after some time blueflakes are separated. By mixing its watery solutions with dilutedhydrochloric or sulfuric acid the color turns nto bluish-green, andafter some time green- 1sh b1ue flakes are separated. It is dissolved byconcentrated sulfuric acid with greenishblue color, which on theaddition of a small quantity of ice water becomes green and turns intoblue, when a greater quantity of water is added. Out of the dilutedsulfuric solution a blue precipitate is separated after some time. It issuitable for dyeing wool with or without the aid of mordants andproduces blue shades with a reddish-hue, which are fast agalnst theaction of washing, fulling, light and alkalies.

My new dye-stuff differs f rom, the product wh ch I have described in aseparate specification, Serial No. 458,902, as the lattercoloring-matter yields blue shades with a greenish hue and results bycombining diazotized aniline and Oleves alphanaphthylamine betamonosulpho acid (beta or delta acid) in equimolecular proportions,rediazotizingandcouphug the so formed diazo compound with one molecularproportion of paratolylalphanaphthylamlne monosulpho acid resulting fromalphanaphthylaminem0110sulpho acid (1:8) and paratoluidine.

Having thus described my invention and in what manner it can beperformed, that which I claim as new, and desire to secure by LettersPatent, is-

1. The process of producing a new coloringmatter by combining equalmolecular proportions of diazotized aniline and Cleves alphaforming anolive-black powder of metallic luster, soluble in ammonia and alcoholwith blue color; almost insoluble in sodium carbonate and soda-lye, evenon heating; insoluble in dilute hydrochloric and sulphuric acids;soluble in water with violet color, which is not changed on addition ofsodium carbonate and ammonia, an excess of these reagents, however,producing a precipitation of blue or reddish-blue flakes, while onaddition of sodalye the aqueous solution becomes dull and separatesafter some time blue flakes, and on addition of dilute hydrochloric orsulphuric acids the aqueous solution turns bluishgreen and separatesafter some time greenish-blue flakes; soluble in concentrated sulphuricacid with greenish-blue color, which on addition of a little ice-waterchanges to greemand on addition of an excess of ice-water turns intoblue and separates after some time a blue precipitate; dyeing wool withor without the aid of mordants reddish blue; and having the qualitiessubstantially as specified.

In testimony whereof I have signed my name in the presence of twosubscribing witnesses.

PI-IILIPP OTT. Witnesses:

W. M. ESSENWEIN, RUDOLPH FRIoKE.

